CN107898828A - Pepper Bi roots of grass compositions dichloromethane extraction position and its preparation method and application - Google Patents
Pepper Bi roots of grass compositions dichloromethane extraction position and its preparation method and application Download PDFInfo
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
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Abstract
The invention belongs to technical field of medicine preparation, is related to medicinal plant chemical composition extraction separation method, and in particular to one kind returns medicine core medicine to pepper Bi roots of grass compositions dichloromethane extraction position and its preparation method and application.The present invention is 1 by weight the Hu Jiao ︰ Bi roots of grass:10‑10:1 weighs pepper, the Bi roots of grass, crushes, and mixes, uses CO2Supercritical extract oil removing, the dregs of a decoction are extracted with 70% ethanol, and extracting solution is concentrated under reduced pressure into no alcohol taste, is extracted with dichloromethane, are recycled the dichloromethane in extract, are obtained liquid extract, dry, obtain dichloromethane extraction position；Dichloromethane extraction contains 10 kinds of compounds such as piperonyl cyclonene butyramide G in position；Pharmacodynamic study the result shows that, pepper Bi roots of grass compositions dichloromethane extract position to rat cerebral ischemia recover early stage there is cerebral protection；Pepper Bi roots of grass compositions dichloromethane extraction position and preparation method thereof has very high science and application value to medicament research and development.
Description
Technical field
The invention belongs to technical field of medicine preparation, is related to medicinal plant chemical composition extraction separation method, and in particular to
One kind returns medicine core medicine to pepper Bi roots of grass compositions dichloromethane extraction position and its preparation method and application.
Background technology
Cerebral apoplexy（stroke）, it is to there is the acute brain of the disturbance of consciousness and focal nerve afunction as common trait
Angiosis.Cerebral Haemorrhage Invasion Rate height, high recurrence rate, disability rate are high, it has also become national dead primary factor.2016《China
Cerebral apoplexy prevention report》More than 200 ten thousand people of patients with cerebral apoplexy is newly sent out in display, China every year；Die of the patient of cerebral apoplexy up to every year
More than 180 ten thousand, living patients also cause deformity mostly, and very big burden is brought to family and society.Chinese Government is every year because of brain
Palsy direct economy pays 37,400,000,000 yuan.With China human mortality aging, getting worse the problem of cerebral apoplexy, society and it is economical will
It can't bear the heavy load（Effect study The 2nd Army Medical College Ph.D. Dissertation .2012s of the quick .ALDH2 of Guo Jin to cerebral arterial thrombosis）.
So far, specific treatment medicine is there is no for cerebral apoplexy, especially to missing golden hour window（6h with
It is interior, thromboembolism treatment）Cerebral arterial thrombosis is treated, and the whole world is still without monolithic standard.The curative of Clinical practice at present
Thing is broadly divided into following a few classes：Thrombolytic drug, medicament for resisting platelet aggregation, drop fine medicine, anticoagulant and nerve protection medicine
Deng.Although these medicines have the effect of certain, but adverse drug reaction is more, and gastrointestinal side effect occurs for some meetings（As Ah
Take charge of a woods）, or the danger of cranium external hemorrhage may be increased（Such as heparin）Even the nerve cell to receive much concern in recent years
Protection medicine also lacks the clinical evaluations such as safety and efficacy（Ren Xuemei, Yang Guang good fortune Cerebral Infarction Treatments present Research and progress
[J] Hebei medicine .2010,16 (2):237-238.）,（The cerebral arterial thrombosis curatives such as Duan Yunxia, Chen little Yu, Zhang Ziqian
Thing progress [J] Central University for Nationalities journal (natural science edition) .2012,21 (2):65-68.）.Therefore, it is true to find curative effect
Cut, safely and effectively Treatment of Cerebral Stroke medicine is extremely urgent.
It is one of Hui ethnic group's rich cultural heritages to return medicine, is the important component of traditional Chinese medicine, quilt in 2008
It is classified as world's nonmaterial culture heritage conservation（《Second batch List of National Intangible Cultural Heritage》977 Ⅸ -17 Hui ethnic group cure
Medicine, 2008）.It is with a long history to return medical treatment cerebral apoplexy,《Huihui Formularies》、《Haiyao Bencao, Oversea Materia Medica》、《Ruizhutang Jingyan Fang, Empirical Recipes from Auspicious Bamboo Hall》Deng warp
The over one hundred head of prescription for the treatment of cerebral apoplexy is included in allusion quotation works, a series of prescriptions represented with Fang Wei in slave think of side, Ha Heili in bundle
It is evident in efficacy according to clinical verification.The research and development of cerebral apoplexy new drug are also Ningxia Hui Autonomous Region 13 period development of national characteristic doctors
The Main way of medicine and big health.
The nearly ripe or mellow fruit of drying that pepper is Piperaceae plant pepper Piper nigrum L..Gas fragrance,
Acrid flavour is peppery.Warming spleen and stomach for dispelling cold, lower gas, dissolving phlegm.The pepper includes white pepper and black pepper.
The nearly ripe or mature fruit cluster of drying that the Bi roots of grass is Piperaceae plant Bi roots of grass Piper longum L..There is special perfume (or spice)
Gas, acrid flavour are peppery.Warming spleen and stomach for dispelling cold, lower gas analgesic.For coldness and pain in the epigastrium, vomiting, diarrhea, cold obstruction causing qi stagnation, chest impediment and cardialgia, headache, tooth
Bitterly.
Modern study achievement shows that pepper, the Bi roots of grass have higher medical value, in cardiovascular system, central nervous system
System, anti-inflammatory, antibacterial, antiviral, liver protection, anticancer etc. are respectively provided with pharmacological activity.
The present invention combines clinical medicine by being excavated, being arranged to time prescription agent that cerebral apoplexy is treated in document at all times
The methods of effect research, determine the composition of " pepper+Bi roots of grass " in the prescription for the treatment of cerebral apoplexy using most, be frequency of occurrence most
Two high taste medicinal materials, the combination frequency of occurrence of " pepper+Bi roots of grass " is 37 times（The such as Li Tingting, Wang Xing, hippology qin returns medicine treatment
Cerebral apoplexy Compatibility Law of TCM Prescriptions studies [J] Chinese experimental pharmacology of traditional Chinese medical formulae magazines, 2013,19 (20):307-311.）.But in the literature
Do not explicitly point out the active component and its pharmaceutical chemistry component for playing therapeutic effect.
In conclusion main problem existing in the prior art has：（1）Although existing treatment cerebral apoplexy medicine has certain treatment
Effect, but adverse drug reaction is more, and searching is curative for effect, safely and effectively Treatment of Cerebral Stroke medicine is extremely urgent；（2）Existing skill
Art points out that the composition of " pepper+Bi roots of grass " is applied at most in the prescription for the treatment of cerebral apoplexy, but is not known and points out to play treatment work
Active component and its pharmaceutical chemistry component.
Therefore, the dichloromethane extraction position to play a role to treating cerebral apoplexy in said composition is furtherd investigate, and is visited
The material base of rope pharmacological activity, is of great significance medicament research and development and quality control.
The content of the invention
For overcome the deficiencies in the prior art, primary and foremost purpose of the invention is to provide a kind of pepper Bi roots of grass composition dichloromethane
Alkane extraction position and preparation method thereof.The preparation method is first by pepper Bi roots of grass composition through Co 2 supercritical fluid method
Oil removing is extracted, then the dregs of a decoction is extracted with ethanol, gained ethanol extract is extracted with dichloromethane, obtains dichloromethane extraction portion
Position.
Second object of the present invention is to provide the purposes at dichloromethane extraction position in pepper Bi roots of grass compositions, that is, is used for
Improve and treat cerebral apoplexy.
Third object of the present invention is to provide the pharmaceutical preparation containing pepper Bi roots of grass compositions dichloromethane extraction position,
For improving and treating cerebral apoplexy.
To achieve the above object, the present invention is achieved through the following technical solutions.
A kind of pepper Bi roots of grass compositions dichloromethane extracts position, it is characterised in that：The dichloromethane extraction position,
Its chemical composition includes：Piperonyl cyclonene butyramide G, piperonyl cyclonene butyramide H, piperonyl cyclonene butyramide C, (2S, 3S) -2- (5- methoxyl groups -
3,4- Methylenedioxybenzyls) -3- (3,4- Methylenedioxybenzyls) butyrolactone, 4- hexyl -4,6- dimethyl -4,5- dihydro pyrroles
Cough up [1,2-A] quinoxaline, N- (5,6,7,8- naphthane -2- bases) acetamide, E-4 (the 15)-β of eudesmene -1,6 α glycol, 3- (3',
4'- methylenedioxyphenyls)-methacrylaldehyde, 7- de-methoxies-egonol -9 (z), 12 (z) linoleic acid, two fourth of phthalic acid
Ester.The present invention is mutually tied using normal phase silica gel column chromatography, anti-phase ODS column chromatographys, LH-20 gel column chromatographies with preparative thin layer chromatography
The method of conjunction has carried out system separation, measure to the chemical composition at dichloromethane extraction position, has obtained above-mentioned 10 kinds of compounds.
Pharmacodynamic experiment the result shows that, above-mentioned 10 kinds of compounds to treatment cerebral apoplexy have it is definite the effect of, to medicament research and development and quality
Control is of great significance.
Further, the preparation method at dichloromethane extraction position is：It is 1 by weight the Hu Jiao ︰ Bi roots of grass:10-10:
1 weighs pepper, the Bi roots of grass, crushes, and mixes, uses CO2Supercritical extract oil removing, the dregs of a decoction are extracted with 70% ethanol, and extracting solution is concentrated under reduced pressure
To no alcohol taste, extracted with dichloromethane, recycle the dichloromethane in extract, obtain liquid extract, it is dry, to obtain the final product.
Further, dichloromethane extraction position can be used for treating cerebral apoplexy.
A kind of preparation method at pepper Bi roots of grass compositions dichloromethane extraction position, it is characterised in that：By weight Hu Jiao ︰
The Bi roots of grass is 1:10-10:1 weighs pepper, the Bi roots of grass, crushes, and mixes, uses CO2Supercritical extract oil removing, the dregs of a decoction are extracted with 70% ethanol,
Extracting solution is concentrated under reduced pressure into no alcohol taste, is extracted with dichloromethane, recycles the dichloromethane in extract, obtains liquid extract, dry, i.e.,
.Wherein, the dichloromethane can use the organic mixed solvent of isopolarity to substitute.
Further, the preparation method comprises the following steps：
S1：CO2Supercritical extract oil removing：It is 1 by weight the Hu Jiao ︰ Bi roots of grass:1 weighs pepper, the Bi roots of grass, puts in pulverizer and crushes,
It is uniformly mixed, uses CO2Supercritical extract is not to fuel-displaced；
S2：Ethanol extracts：The dregs of a decoction after oil are removed, are extracted with 70% ethanol, merges extracting solution, is concentrated under reduced pressure into no alcohol taste, obtains second
Alcohol crude extract solution；
S3：Dichloromethane extracts：Alcohol extracts solution is taken, adds isometric dichloromethane, is extracted, stratification, collects two
Chloromethane alkane extract, is recovered under reduced pressure dichloromethane, dry, and position, sealed storage are extracted up to dichloromethane.
In step sl, the CO2The process conditions of supercritical extract are：Extraction kettle pressure 300Bar, 55 DEG C of temperature；Point
From kettle I pressure 80Bar, separation reactor I temperature 50 C；40 DEG C of separation reactor I I pressure 60Bar, separation reactor I I temperature.
In step s 2, the process conditions of the 70% ethanol extraction are：Extraction time is 3 times, each 3h, Yao Zha ︰ 70%
The volume ratio of ethanol is 1:9-1:11.
In step s3, the method for the addition dichloromethane extraction is：Shaking out or continuous countercurrent extraction, wherein shaking
The process conditions for shaking extraction are that process conditions are：Every batch of extraction times are no less than 4 times, combined dichloromethane extract；It is described close
The temperature of envelope storage is -10 DEG C~0 DEG C, is preferably -4 DEG C.
Further, the preparation method can be used for the preparation of the medicine for the treatment of cerebral apoplexy.
The pharmaceutical preparation at position is extracted containing a kind of pepper Bi roots of grass compositions dichloromethane as claimed in claim 1, its
It is characterized in that：It is processed into by the dichloromethane extraction position and the auxiliary material for meeting medicinal requirements, wherein dichloromethane extracts
It is 1 to take the weight ratio of position and auxiliary material:0.2-1:5.
Further, the pharmaceutical preparation is dispersible tablet, soft capsule, dripping pill, ordinary tablet, hard shell capsules, granule, mouth containing
Piece, injection etc..When pharmaceutical preparation for dispersible tablet, granule, hard shell capsules, pill, ordinary tablet buccal tablet when solid pharmaceutical preparation when,
The auxiliary material includes antiplastering aid, diluent（Filler）, flavouring, disintegrant, glidant, lubricant, wherein antiplastering aid is D-
It is mannitol, talcum powder, mineral oil, pungent, in glycerol decanoate and starch Sodium Octenyl Succinate any one or a few
Combination；Wherein diluent is any one or a few the group in xylitol, D-mannital, D-sorbite, microcrystalline cellulose
Close；Wherein flavouring is Sucralose, Momordia grosvenori aglycone, Aspartame, glycyrrhizin, stevioside, honey element, citric acid, apple
Any one or the combination of several of them in acid, tartaric acid, fumaric acid, flavoring pineapple essence, strawberry essence, flavoring orange essence, Mint Essence；
Wherein disintegrant is crospovidone, in sodium carboxymethyl starch, Ac-Di-Sol, low-substituted hydroxypropyl cellulose
One or more of combinations；Wherein glidant is colloidal silica；Wherein lubricant is magnesium stearate, talcum powder, dodecane
One or more of combinations in base sodium sulphate；When needing, water can be added as adhesive.When pharmaceutical preparation is soft capsule,
The auxiliary material includes matrix, dispersant, suspending agent, preservative, its mesostroma includes glycerine, gelatin etc., and dispersant includes salad
Oil, corn oil, polyethylene glycol 400, Macrogol 600 or PVPK30 etc., suspending agent include paraffin, beeswax, Macrogol 4000,
Macrogol 6000 etc., preservative are methyl p-hydroxybenzoate（1.6%）And P-hydroxybenzoic acid and ester（0.04%）Mixing
Thing；When pharmaceutical preparation is dripping pill, the auxiliary material include matrix, condensate liquid, its mesostroma stearic acid, glycerin monostearate,
The combination of any one or more in insect wax, hydrogenated vegetable oil, stearyl alcohol, cetanol, semi-synthetic fatty acid ester, condensate liquid are liquid
Any one in body paraffin, ethanol solution or dilute acid soln.
Beneficial effects of the present invention：
The present invention extracts pepper Bi roots of grass composition carbon dioxide supercritical extraction oil removing, the dregs of a decoction with 70% ethanol, and extracting solution subtracts
Pressure is concentrated into no alcohol taste, is extracted with dichloromethane, recycles the dichloromethane in extract, dry, obtains dichloromethane extraction portion
Position；The present invention will also using normal phase silica gel column chromatography, anti-phase ODS column chromatographys, LH-20 gel column chromatographies and preparative thin layer chromatography
The chemical composition at dichloromethane extraction position carries out system separation, measure, obtains 10 kinds of compounds；Dichloromethane extracts position pair
Rat cerebral ischemia recover early stage protective effect test result indicates that, pepper, the Bi roots of grass dichloromethane extraction position rat brain is lacked
Blood recovers have cerebral protection in early days, shows as the reduction of nervous function neurological deficit score, and beam walking ability is recovered, Yi Jiqian
Limb grip strength improves；Pharmacodynamic experiment the result shows that, from pepper, the Bi roots of grass dichloromethane extraction position in separation, purifying obtain
10 kinds of compounds to treatment cerebral apoplexy have it is definite the effect of, be of great significance to medicament research and development and quality control.
Embodiment
Technical scheme is described in detail below, but the implementation of the present invention is not limited thereto.
Embodiment 1：
A kind of pepper Bi roots of grass compositions dichloromethane extracts position, and its preparation method comprises the following steps：
S1：CO2Supercritical extract oil removing：Pepper, each 20kg of the Bi roots of grass are weighed, puts in pulverizer and crushes, is uniformly mixed, puts into CO2
Not fuel-displaced, extraction conditions is extracted in supercritical extraction reactor：Pressure 300Bar；55 DEG C of temperature, separation reactor I pressure 80Bar, separation
I temperature 50 Cs, separation reactor I I pressure 60Bar, 40 DEG C of separation II temperature.
S2：Ethanol extracts：The dregs of a decoction obtained by step S1 are added in multi-function extractor several times, are carried with 70% ethanol
3 times, each 3h are taken, the dregs of a decoction: the volume ratio of 70% ethanol is 1:10.Merge extracting solution, put in Rotary Evaporators, be threaded to no alcohol taste,
Obtain alcohol extracts solution.
S3：Dichloromethane extracts：By the alcohol extracts solution obtained by step S2 and dichloromethane with volume ratio 1:1
Ratio mixes, and adds separatory funnel, shakes up, stratification, collects dichloromethane extract；Every batch of extraction times are no less than 4 times,
Combined dichloromethane extract, recycles the dichloromethane in dichloromethane extract with Rotary Evaporators, obtains liquid extract.Take out stream
Medicinal extract, spontaneously dries, and position is extracted up to dichloromethane；Sealed storage, storage temperature are -4 DEG C.
Embodiment 2：
On the basis of embodiment 1, the dichloromethane extraction position obtained from embodiment 1 is carried out recovering early to rat cerebral ischemia
The protective effect experiment of phase.
1 experiment material
1.1 main agents and consumptive material
A4-2026 line bolts；Chloraldurate；95% alcohol；Distilled water；Sodium carboxymethylcellulose（CMC-Na）；Malonaldehyde MDA is examined
Test agent box.
1.2 key instrument
The big mouse grip testers of YLS-12A；Electronic analytical balance.
2. experimental animal and method
Male and healthy SD rats, 280 ~ 320g of weight, is provided by Ningxia Medical University's Experimental Animal Center.
Block artery in rat with line brush, establish rat permanent cerebral ischemia damage model.Surgery models are successful
Rat is grouped at random（Every group of 10-15 rat）：Model group, sham-operation group, dichloromethane extraction position are high（200mg/kg）, it is low
Dosage group（100mg/kg）.The gastric infusion after 6 h of cerebral ischemia, 1 time/d, is administered 14 days.By monitor 3d, 6d, 9d, 12d and
14d rat body weights, attitudinal reflex, body swing, beam walking, forelimb grip value Assessment of Changes dichloromethane extraction position are played a game
The influence of the neurobehavioral of stove cerebral ischemia rat.
2.1 weight detect
3 d, 6 d, 9 d, 12 d and 14 d measure rat body weights after pMCAO modelings.
2.2 Neuroscore.
2.2.1 attitudinal reflex is tested
3 d, 6 d, 9 d, 12 d and 14 d after pMCAO modelings, comment animal according to 5 grades of point systems of Longa
Point：0 point：Put forward rat-tail and leave about 1 m of ground, observe forelimb flexing situation, the double forelimbs of normal rat symmetrically stretch to ground；1 point：Hand
There is wrist flexing, elbow flexing, shoulder inward turning or existing wrist in art offside forelimb, the flexing of elbow has shoulder inward turning person again；2 points：Animal is put
Moved on plane earth, pushing away both shoulders respectively to offside, the mouse of normal or slight functional disturbance is all unequal in the two directions
Ground slides, and the rat resistance of severe dysfunction is persistently reduced；3 points：Rat does not to the left turn-take ceaselessly person.
2.2.2 body swing is tested
Lifted rat-tail away from ground 1m at, score respectively in the 3rd d, 6 d, 9 d, 12 d and 14 d it.Standards of grading：0
Point：Trunk is swung left and right；1 point：Asymmetry is waved less than 30 degree；2 points：Asymmetry is waved more than 30 degree.
2.2.3 beam walking test
Beam grows 120 cm, wide 2.0 cm, away from the horizontal hanging placements of 80 cm of ground.Beam one end connects one 20 × 20 × 20
Cm magazines, beam is passed to appropriate stimulation in rats.Preoperative exercise 7d, 3 d, 6 d, 9 d, 12 after pMCAO modelings
D and 14 d is detected for observing time point.
Standards of grading：6 points：Pass through；5 points：By, but damage side hind leg and slide 1 time；4 points：Slide more than 1 time but
Less than total step number 50%；3 points：Slide number and exceed total step number 50%；2 points：Attempt by beam, but thrown from beam；1 point：
It can repose on beam but can not move；0 point：It cannot repose on beam, directly be thrown from beam.
2.2.4 forelimb grip is tested
The size of grip strength test evaluation rat cerebral ischemia right fore grip strength.Tester puies forward rat-tail, and rat is placed in drawing
Power instrument test zone.When tester hold rat-tail pull rat backward when, rat attempt with forelimb grasp cross bar do not put so as not to from
Cross bar slips.Continue to pull rat, until rat slips, read the maximum pull value for slipping rat.Respectively at pMCAO modelings
3 d, 6 d, 9 d, 12 d and 14 d are detected for observing time point afterwards.
3. experimental result
3. 1 pepper Bi roots of grass dichloromethane extracts influence of the position to pMCAO rat body weights
As shown in 1 result of table, compared with model group, sham-operation group pMCAO rat body weights are significantly raised at 3 ~ 14 days（P<
0.01）；Dichloromethane extracts position low dose group（100 mg/kg）PMCAO rat body weights were showed no 3 ~ 14 days positions substantially to be changed
Become；Dichloromethane extracts position high dose group（200 mg/kg）PMCAO rat body weights are significantly raised at 6 ~ 14 days（P<
0.01）.
Note：Compared with model group,# P<0.05；## P<0.01；*P<0.05；**P<0.01（nModel group=11；nSham-operation group=
13；nDCM 100 mg/kg=9；nDCM 200 mg/kg=9）.
3.2 pepper Bi roots of grass dichloromethane extract influence of the position to pMCAO rat nerve functions
3.2.1 influence of the pepper Bi roots of grass dichloromethane extraction position to pMCAO rat attitudinal reflexes
As shown in 2 result of table, compared with model group, sham-operation group pMCAO rats attitudinal reflex was showed no rise at 3 ~ 14 days（P<
0.01）；Dichloromethane extracts position low dose group（100 mg/kg）PMCAO rats attitudinal reflex obvious drop at 6,9,12 days
It is low（P<0.05；P<0.01）；Dichloromethane extracts position high dose group（200 mg/kg）The attitudinal reflex of pMCAO rats 9,
12nd, obvious reduction in 14 days（P<0.01）.
Note：Compared with model group,# P<0.05；## P<0.01；*P<0.05；**P<0.01（nModel group=11；nSham-operation group=
13；nDCM 100 mg/kg=9；nDCM 200 mg/kg=9）.
3.2.2 the influence that pepper Bi roots of grass dichloromethane extraction position swings pMCAO rat bodies
As shown in table 3, compared with model group, sham-operation group pMCAO rat bodies are swung was showed no rise at 3 ~ 14 days（P<
0.01）；Dichloromethane extracts position low dose group（100 mg/kg）PMCAO rat bodies swing obvious at 3,6,9,14 days
Reduce（P<0.05；P<0.01）；Dichloromethane extracts position high dose group（200 mg/kg）PMCAO rat bodies swing 3,
9th, obvious reduction in 12,14 days（P<0.01）.
Note：Compared with model group,# P<0.05；## P<0.01；*P<0.05；**P<0.01（nModel group=11；nSham-operation group=
13；nDCM 100 mg/kg=9；nDCM 200 mg/kg=9）.
3.2.3 influence of the pepper Bi roots of grass dichloromethane extraction position to pMCAO rat beam walkings
As shown in 4 result of table, compared with model group, sham-operation group pMCAO rats beam walking was showed no reduction at 3 ~ 14 days（P<
0.01）；Dichloromethane extracts position low dose group（100 mg/kg）PMCAO rats beam walking is significantly raised at 6,12 days
（P<0.05）；Dichloromethane extracts position high dose group（200 mg/kg）PMCAO rats beam walking is significantly raised at 3 ~ 14 days
（P<0.01）.
Note：Compared with model group,# P<0.05；## P<0.01；*P<0.05；**P<0.01（nModel group=11；nSham-operation group=
13；nDCM 100 mg/kg=9；nDCM 200 mg/kg=9）.
3.2.4 influence of the pepper Bi roots of grass dichloromethane extraction position to pMCAO rat grips
As can be seen from the results of table 5, compared with model group, sham-operation group pMCAO rat grip values had significant at 3 ~ 14 days
（P<0.01）;Dichloromethane extracts position low dose group（100 mg/kg）PMCAO rat grip values are significantly raised at 6 days（P<
0.01）;Dichloromethane extracts position high dose group（200 mg/kg）PMCAO rat grip values are significantly raised at 3 ~ 14 days（P<
0.05；P<0.01）.
Note：Compared with model group,# P<0.05；## P<0.01；*P<0.05；**P<0.01（nModel group=11；nSham-operation group=
13；nDCM 100 mg/kg=9；nDCM 200 mg/kg=9）.
4. conclusion
After rat pMCAO modelings, sham-operation group survival rate 100% after 14 days；Dichloromethane extraction position is high（200mg/kg）, it is low
Dosage group（100mg/kg）Survival rate after 14 days（81.82% and 75.00%）It is higher than model group（73.33%）.Pepper, the Bi roots of grass two
Chloromethanes extracts position and recovers have cerebral protection in early days in rat cerebral ischemia, shows as nervous function neurological deficit score drop
Low, beam walking ability is recovered and forelimb grip strength improves.
Embodiment 3
The preparation of conventional tablet：
The dichloromethane extraction position for obtaining embodiment 1 on the basis of embodiment 1 and auxiliary material are 1 by weight:5 mixing,
Granulation, tabletting, to obtain the final product.
Embodiment 4
The preparation of dispersible tablet：
The dichloromethane extraction position for obtaining embodiment 1 on the basis of embodiment 1 and auxiliary material are 1 by weight:1 mixing,
Crush, cross 180 mesh sieves, pelletize, tabletting, to obtain the final product.
Embodiment 5
The preparation of capsule, granule：
The dichloromethane extraction position for obtaining embodiment 1 on the basis of embodiment 1 and auxiliary material are 1 by weight:1 mixing,
Capsule or granule is made, to obtain the final product.
The above, is only presently preferred embodiments of the present invention, and is not used to the interest field of the limitation present invention.It is any with this
The technical solution that the interest field that claim is covered is implemented, or any those skilled in the art, utilize
The method content of the disclosure above makes the scheme of many possible changes and modifications, belongs to protection scope of the present invention.
Claims (10)
1. a kind of pepper Bi roots of grass compositions dichloromethane extracts position, it is characterised in that：The dichloromethane extraction position, its
Chemical composition includes：Piperonyl cyclonene butyramide G, piperonyl cyclonene butyramide H, piperonyl cyclonene butyramide C, (2S, 3S) -2- (5- methoxyl group -3,
4- Methylenedioxybenzyls) -3- (3,4- Methylenedioxybenzyls) butyrolactone, 4- hexyl -4,6- dimethyl -4,5- pyrrolin
[1,2-A] quinoxaline, N- (5,6,7,8- naphthane -2- bases) acetamide, E-4 (the 15)-β of eudesmene -1,6 α glycol, 3- (3',
4'- methylenedioxyphenyls)-methacrylaldehyde, 7- de-methoxies-egonol -9 (z), 12 (z) linoleic acid, two fourth of phthalic acid
Ester.
A kind of 2. pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 1, it is characterised in that：Described two
Chloromethanes extraction position preparation method be：It is 1 by weight the Hu Jiao ︰ Bi roots of grass:10-10:1 weighs pepper, the Bi roots of grass, crushes, and mixes
It is even, use CO2Supercritical extract oil removing, the dregs of a decoction are extracted with 70% ethanol, and extracting solution is concentrated under reduced pressure into no alcohol taste, is extracted with dichloromethane
Take, recycle the dichloromethane in extract, obtain liquid extract, it is dry, to obtain the final product.
A kind of 3. pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 1, it is characterised in that：Described two
Chloromethanes extraction position can be used for treating cerebral apoplexy.
A kind of 4. preparation method at pepper Bi roots of grass compositions dichloromethane extraction position, it is characterised in that：By weight Hu Jiao ︰ Bi
The roots of grass is 1:10-10:1 weighs pepper, the Bi roots of grass, crushes, and mixes, uses CO2Supercritical extract oil removing, the dregs of a decoction are extracted with 70% ethanol, carried
Take liquid to be concentrated under reduced pressure into no alcohol taste, extracted with dichloromethane, recycle the dichloromethane in extract, obtain liquid extract, it is dry, i.e.,
.
5. a kind of preparation method at pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 4, its feature exist
In：The preparation method comprises the following steps：
S1：CO2Supercritical extract oil removing：It is 1 by weight the Hu Jiao ︰ Bi roots of grass:1 weighs pepper, the Bi roots of grass, puts in pulverizer and crushes, and mixes
Close uniformly, use CO2Supercritical extract is not to fuel-displaced；
S2：Ethanol extracts：The dregs of a decoction after oil are removed, are extracted with 70% ethanol, merges extracting solution, is concentrated under reduced pressure into no alcohol taste, obtains second
Alcohol crude extract solution；
S3：Dichloromethane extracts：Alcohol extracts solution is taken, adds isometric dichloromethane, is extracted, stratification, collects two
Chloromethane alkane extract, is recovered under reduced pressure dichloromethane, dry, and position, sealed storage are extracted up to dichloromethane.
6. a kind of preparation method at pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 4, its feature exist
In：
In step sl, the CO2The process conditions of supercritical extract are：Extraction kettle pressure 300Bar, 55 DEG C of temperature；Separation reactor I
Pressure 80Bar, separation reactor I temperature 50 C；40 DEG C of separation reactor I I pressure 60Bar, separation reactor I I temperature；
In step s 2, the process conditions of the 70% ethanol extraction are：Extraction time is 3 times, each 3h, Yao Zha 70% ethanol of ︰
Volume ratio be 1:9-1:11；
In step s3, the method for the addition dichloromethane extraction is：Shaking out or continuous countercurrent extraction, wherein shaking extraction
The process conditions taken are that process conditions are：Every batch of extraction times are no less than 4 times, combined dichloromethane extract；The sealing storage
The temperature deposited is -10 DEG C~0 DEG C.
7. a kind of preparation method at pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 4, its feature exist
In：The dichloromethane can use the organic mixed solvent of isopolarity to substitute.
8. a kind of preparation method at pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 4, its feature exist
In：The preparation method can be used for the preparation of the medicine for the treatment of cerebral apoplexy.
9. containing a kind of pharmaceutical preparation at pepper Bi roots of grass compositions dichloromethane extraction position as claimed in claim 1, it is special
Sign is：It is processed into by the dichloromethane extraction position and the auxiliary material for meeting medicinal requirements, wherein dichloromethane extracts
The weight ratio of position and auxiliary material is 1:0.2-1:5.
10. as claimed in claim 9 contain a kind of pepper Bi roots of grass composition dichloromethane extraction portion as claimed in claim 1
The pharmaceutical preparation of position, it is characterised in that：The pharmaceutical preparation is dispersible tablet, soft capsule, dripping pill, ordinary tablet, hard shell capsules, particle
Agent, buccal tablet, injection.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711234142.4A CN107898828A (en) | 2017-11-30 | 2017-11-30 | Pepper Bi roots of grass compositions dichloromethane extraction position and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711234142.4A CN107898828A (en) | 2017-11-30 | 2017-11-30 | Pepper Bi roots of grass compositions dichloromethane extraction position and its preparation method and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702520A (en) * | 2021-08-17 | 2021-11-26 | 中南民族大学 | Method for controlling quality of long pepper medicinal material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106913628A (en) * | 2015-12-24 | 2017-07-04 | 宁夏医科大学 | Treatment cerebral ischemia active site medicine and preparation method based on pepper and Piper longum |
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2017
- 2017-11-30 CN CN201711234142.4A patent/CN107898828A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106913628A (en) * | 2015-12-24 | 2017-07-04 | 宁夏医科大学 | Treatment cerebral ischemia active site medicine and preparation method based on pepper and Piper longum |
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| Title |
|---|
| BING WANG等: "Anti-inflammatory activity and chemical composition of dichloromethane extract fromPiper nigrum and P. longum on permanent focal cerebral ischemia injury in rats", 《REVISTA BRASILEIRA DE FARMACOGNOSIA》 * |
| 吴霞等: "荜拔化学成分的研究（I）", 《中草药》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702520A (en) * | 2021-08-17 | 2021-11-26 | 中南民族大学 | Method for controlling quality of long pepper medicinal material |
| CN113702520B (en) * | 2021-08-17 | 2022-09-16 | 中南民族大学 | Method for controlling quality of long pepper medicinal material |
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